Synthesis Process, Structure Characterization And Performance Study Of Dihydroxylammonium5,5’-Bistetrazole-1,1’-diolate

As the precision of the weapons equipment, large-size of the weapons platform andchange of pattern in the modern war, the requirement of weapon warhead increases, whichmakes the single-compound explosive not only have the ideal level of energy more need goodsafety performance. The Dihydroxylammonium5,5’-Bistetrazole-1,1’-diolate (TKX50) havehigh energy level which as the same level as HNIW, and the mechanical sensitivity of theTKX50is very low, which fit the requirements of the modern war for the performance of thesingle-compound explosive, as a kind of high-energy insensitive single-compound explosives,it have extremely application value. In this paper, synthesis process and properties of theTKX50were studied.A new synthesis route of TKX50was designed and the synthesis process wasoptimized. With glyoxal as raw material, TKX50was synthesized in4steps with72.5%total yield, the reaction include oximation, chlorination, azidation, cyclization and salification.The effect of the feeding temperature and reaction time on the oximation reaction yield wereinvestigated. When the feed temperature is0℃and reaction time is12h, yield is the highestwhich is93.2%. Invented "one pot method" to get diazidoglyoxime, which merge thechlorination and azidation into one step. The effect of the feeding temperature and reactiontime on the "one pot method" yield were investigated. Chlorinated agent A was added at0℃and react12h at room temperature, NaN3was added at0℃and react1h at0℃, yield isthe highest, which is85.4%. The effect of the reaction temperature and reaction time on theyield of1,1-BTO were investigated. When the reaction temperature is0℃and reaction timeis12h, yield is the highest which is87.4%. The structure of TKX-50and intermediateproducts were characterized by IR,1H NMR,13C NMR. The single crystal ofdiazidoglyoxime,1,1-BTO, and TKX-50was cultivated, molecular structures was elucidated by single-crystal X-ray diffraction.The thermal decomposition action of diazidoglyoxime,1,1-BTO, SBTD.4H2O and TKX-50were investigated. At the heating rate of10.0K/min, the decomposition peak of diazidoglyoxime and1,1-BTO is179.05℃and243.13℃respectively. The thermal decomposition process of SBTD·4H2O consisted of two stages, the first peak is402.18℃and the second is550.98℃. The thermal decomposition process of TKX-50also consisted of two stages, the first peak is402.18℃and the second is550.98℃. The thermal decomposition kinetics of the first stage of TKX-50was investigated. The activation energy and pre-exponential factor for the first stage is147.05kJ/mol and1012.91S-1respectively. Thermal decomposition of the first stage is controlled by the mechanism of2D diffusion, and the reaction mechanism obey the equation of Jander. The kinetics equation for the first decomposition stage may be expressed asThe critical temperature of thermal explosion of TKX-50is499.46K, which higher than RDX(490.5K), the thermal safety performance is fine. The compatibility of TKX-50with several common explosive mixture composition was investigated by thermal analysis technology. The results show that TKX-50have good compatibility with90#wax, F2311and Estane5702. According to the GJB772A-1997, the mechanical sensitivity of TKX-50were tested, the friction and impact explosion percentage is both0%, which is far below the HNIW.